CN109092356A - 一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法 - Google Patents
一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法,其是采用固相法合成五并苯醌,并选取乙二胺诱导五并苯醌形成组装体,再将该组装体分散在溶剂中与硝酸银溶液进行水浴反应,使银纳米粒子均匀分布在乙二胺诱导五并苯醌组装体的表面上,即获得复合催化剂。本发明所制备的乙二胺诱导五并苯醌组装体负载纳米银复合催化剂能够显著促进对二甲戊乐灵的催化还原性能。
Description
技术领域
本发明属于纳米材料改性技术领域,涉及一种新型纳米复合催化剂的制备方法,具体涉及一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法。
背景技术
随着现代农业的迅速发展,化学肥料和农药的大量使用对我们赖以生存的环境造成了日益严重的污染,也在潜移默化中损害着人类的身体健康。随着科学与科技的发展,处理废水中的污染物一般有以下几种方法:吸附法、催化还原法、凝固过滤法、离子交换法、渗透法、化学沉淀法、臭氧氧化法、生物降解法以及超声波处理法。其中催化还原法是最为普遍且成效较快的一种方法。由于金属催化剂在污水处理及净化技术方面展现出优异的性能,使得金属纳米颗粒催化还原技术得到了广泛的关注。
常用的金属纳米材料有金纳米颗粒、银纳米颗粒、钯纳米颗粒、铂纳米颗粒、铜纳米颗粒和镍纳米颗粒。与其他的金属相比,银纳米颗粒具有一定的优异性:(1)银纳米颗粒的催化活性与其纳米颗粒尺寸息息相关,同时银纳米颗粒的尺寸相比于其他金属可控性更强;(2)银纳米颗粒的复合材料在温和的条件下,如室温或者更低温度,依旧可以表现出极好的催化性能;(3)相比于与其他金属的复合材料,银纳米颗粒复合材料具有更高的选择性、更加优异的稳定性与可重复性,同时制作成本相对低廉。但小尺寸的银纳米颗粒具备较大的比表面积,使得银纳米颗粒极易发生团聚现象,而团聚的银纳米颗粒将降低甚至失去催化活性。因此如何有效的抑制银纳米颗粒的团聚对银纳米颗粒的性能尤为重要。
五并苯醌是一种新型的具有潜力的有机小分子半导体材料,其对于污染物具有较好的摩尔吸附性能,可以很好的吸附分散体系中的污染物,从而提高催化性能。五并苯醌具有大的平面结构和π-π共轭的电子体系,使得整体分子相较于其他一些具有相同性质的有机分子在热稳定性、光稳定性和化学稳定性上有更突出的表现。通过乙二胺回流可诱导五并苯醌组装形成片状结构。以五并苯醌作为载体,可以将银稳定在纳米尺度,从而提高纳米银的催化活性。同时,五并苯醌具有较强的电子传输能力,可在一定程度上进一步提升纳米银的催化活性。
发明内容
本发明的目的及所要解决的技术问题是提供一种稳定的乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法。
本发明解决技术问题,采用如下技术方案:
本发明公开了一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法,其特点在于,包括如下步骤:
步骤1、以邻苯二甲醛与1,4-环己二酮为原料,研磨条件下加入KOH溶液,所得产物洗涤干燥后获得五并苯醌;
步骤2、称取100~1200mg五并苯醌和30~35mL乙二胺置于单口烧瓶中,超声使五并苯醌分散均匀,然后将烧瓶置于130℃油浴锅中,冷凝回流条件下匀速搅拌5-15h,所得产品洗涤、干燥后,获得乙二胺诱导五并苯醌组装体;
步骤3、取40~50mg步骤2所得乙二胺诱导五并苯醌组装体加入在20-50mL体积浓度为50%的乙醇溶液中,超声分散均匀,形成反应体系;
取0.1~1mL 1mol/L的硝酸银溶液分散在15mL去离子水中,然后逐滴加入至反应体系中,室温搅拌反应3~12h;
再取占硝酸银摩尔质量2.5~3倍的NaBH4溶于15mL的去离子水中,然后逐滴加入至反应体系中,继续搅拌反应12~18h;
反应结束后,所得产物经离心洗涤、干燥,即获得乙二胺诱导五并苯醌组装体负载纳米银复合催化剂。
优选的,步骤1所述五并苯醌的具体制备方法如下:称取1~1.31g邻苯二甲醛和0.45~0.50g1,4-环己二酮于研钵中研磨,使其混合均匀并继续研磨至类凝胶状;然后滴加10~15mL质量浓度为15%的KOH溶液,边滴加边研磨,产生沉淀物;以12000r/min离心15~20min,从未反应的原料中分离出产物;所得产物经离心清洗、冷冻干燥,即获得五并苯醌。
与已有技术相比,本发明的有益效果体现在:
本发明的复合催化剂以乙二胺诱导五并苯醌组装体作为载体,将银稳定在纳米尺度,提高了纳米银自身的催化活性;本发明所制备的复合催化剂能够显著促进二甲戊乐灵的催化性能。
附图说明
图1为乙二胺诱导五并苯醌组装体的扫描电镜图。
图2为乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的透射电镜图。
图3为乙二胺诱导五并苯醌组装体与乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的X射线衍射谱图。
图4为乙二胺诱导五并苯醌组装体与乙二胺诱导五并苯醌组装体负载纳米银复合催化剂催化二甲戊乐灵的残留比与时间图。
具体实施方式
下面结合附图和实施例对本发明作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
本实施例首先按如下步骤合成乙二胺诱导五并苯醌组装体负载纳米银复合催化剂:
(1)称取1.31g邻苯二甲醛和0.50g 1,4-环己二酮于研钵中研磨,使其混合均匀并继续研磨0.5h,至类凝胶状;然后缓慢滴加15mL质量浓度为15%的KOH溶液,边滴加边研磨,产生黄色沉淀物。接着将产物以12000r/min离心20min,从未反应的原料中分离出需要的产物。所得产物经离心清洗、冷冻干燥,即获得五并苯醌。
(2)取100mg的五并苯醌和30~35mL乙二胺置于单口烧瓶中,超声辅助分散30min。完全分散后,搭建冷凝回流装置,将油浴锅温度设置为130℃。冷凝回流条件下匀速恒温搅拌10h,自然冷却至室温。所得产品依次用水和乙醇离心洗涤多次,再经冷冻干燥,即获得乙二胺诱导五并苯醌组装体。
图1为乙二胺诱导五并苯醌组装体的扫描电镜图,产物为纳米片状结构,形貌均匀。
(3)取45mg的乙二胺诱导五并苯醌组装体加入在30mL体积浓度为50%的乙醇水溶液中,超声处理30min确保乙二胺诱导五并苯醌组装体均匀分散在溶液中,形成反应体系。
用移液枪准确移取0.46mL 1.0mol/L的硝酸银溶液分散在15mL去离子水中。将分散好的硝酸银溶液逐滴加入到反应体系中,在室温条件下持续搅拌12h,确保银离子被乙二胺诱导五并苯醌组装体所吸附完全。
取3倍摩尔质量与硝酸银的NaBH4溶于15mL的去离子水中,然后逐滴加入至反应体系中,持续搅拌一夜。
反应结束后,所得产物依次使用去离子水与无水乙醇洗涤多次,除去反应体系中未反应的原料以及反应产生的副产物,再经冷冻干燥,即获得乙二胺诱导五并苯醌组装体负载纳米银复合催化剂。
图2为本实施例所得催化剂的透射电镜图,可以看出银已被还原成较均一的纳米粒子,并均匀地分布在乙二胺诱导五并苯醌组装体上。图3为本实施例所得催化剂的X射线衍射谱图(其中,曲线0表示乙二胺诱导五并苯醌组装体的X射线衍射谱图,曲线1线表示乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的X射线衍射谱图),可以看得出成功合成了乙二胺诱导五并苯醌组装体负载纳米银复合催化剂。
为验证本实施例所得催化剂的性能,进行如下测试:取4mg乙二胺诱导五并苯醌组装体负载纳米银复合催化剂分散在10mL 100ppm(1mg/L=1ppm)二甲戊乐灵甲醇溶液中,黑暗下超声处理30min,确保样品均匀分散在溶液中。室温下,磁力搅拌2h,确保催化剂与二甲戊乐灵之间达到吸附-解吸附平衡。然后在快速搅拌的条件下,快速加入30mL 0.1mol/L的NaBH4水溶液,每间隔合适的时间,通过针式过滤器将乙二胺诱导五并苯醌组装体负载纳米银复合催化剂与溶液分离。通过分光光度计测试二甲戊乐灵吸收峰峰值的变化,以确定催化剂催化效果。采用相同的方法检测乙二胺诱导五并苯醌组装体的催化效果,以进行对比。
如图4所示,为乙二胺诱导五并苯醌组装体负载纳米银复合催化剂催化二甲戊乐灵的残留比与时间图(其中,曲线0表示乙二胺诱导五并苯醌组装体催化二甲戊乐灵的残留比与时间图;曲线1表示乙二胺诱导五并苯醌组装体负载纳米银复合催化剂催化二甲戊乐灵的残留比与时间图),可见本发明的复合催化剂对催化还原对硝基苯酚反应有优异的催化活性。
以上仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种乙二胺诱导五并苯醌组装体负载纳米银复合催化剂的制备方法,其特征在于,包括如下步骤:
步骤1、以邻苯二甲醛与1,4-环己二酮为原料,研磨条件下加入KOH溶液,所得产物洗涤干燥后获得五并苯醌;
步骤2、称取100~1200mg五并苯醌和30~35mL乙二胺置于单口烧瓶中,超声使五并苯醌分散均匀,然后将烧瓶置于130℃油浴锅中,冷凝回流条件下匀速搅拌5-15h,所得产品洗涤、干燥后,获得乙二胺诱导五并苯醌组装体;
步骤3、取40~50mg步骤2所得乙二胺诱导五并苯醌组装体加入在20-50mL体积浓度为50%的乙醇溶液中,超声分散均匀,形成反应体系;
取0.1~1mL 1mol/L的硝酸银溶液分散在15mL去离子水中,然后逐滴加入至反应体系中,室温搅拌反应3~12h;
再取占硝酸银摩尔质量2.5~3倍的NaBH4溶于15mL的去离子水中,然后逐滴加入至反应体系中,继续搅拌反应12~18h;
反应结束后,所得产物经离心洗涤、干燥,即获得乙二胺诱导五并苯醌组装体负载纳米银复合催化剂。
2.根据权利要求1所述的制备方法,其特征在于:步骤1所述五并苯醌的具体制备方法如下:
称取1~1.31g邻苯二甲醛和0.45~0.50g 1,4-环己二酮于研钵中研磨,使其混合均匀并继续研磨至类凝胶状;然后滴加10~15mL质量浓度为15%的KOH溶液,边滴加边研磨,产生沉淀物;以12000r/min离心15~20min,从未反应的原料中分离出产物;所得产物经离心清洗、冷冻干燥,即获得五并苯醌。
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